関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Cyclohexylsulfamyl chloride | HCID 12914615 | — |
| 反応物 | Methyl N-(iminomethoxymethyl)carbamate | HCID 137319931 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-Carbomethoxy-N-cyclohexylsulfamyl-O-methylisourea | HCID 21269103 | — |
反応手順
Triethylamine (112 g) is added to a stirred solution of N-carbomethoxy-O-methylisourea (132.1 g) in anhydrous THF (900 ml). The solution is cooled to -70° C. under an N2 atmosphere and solution of cyclohexylsulfamoyl chloride (198 g) in anhydrous THF (400 ml) is added dropwise to the reaction mixture. The reaction mixture is warmed to RT filtered through Celite®, washed with anhydrous THF and evaporated to yield an oil which is taken up in methylene chloride, washed with 0.5N HCl and allowed to stand overnight. The organic layer is washed with 0.5N HCl, dried, filtered, washed with methylene chloride, evaporated and dried under high vacuum affording the desired product as an oil which is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04704388 |
|---|
| 出典データセット | uspto-grants-1987_11 |
|---|
| ORD ID | ord-255c3752580c4567bd3b121ac161a56e |
|---|
| 出典メモ | uspto-grants-1987_11 |
|---|